Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | RU 25591 | HCID 182578 | — |
| Catalyst | Adams' catalyst | HCID 345198 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | HCID 178418361 | HCID 178418361 | — |
| Product | HCID 21153170 | HCID 21153170 | 107.1% |
Reaction Steps
370 mg of platinum dioxide were added to a solution of 3.7 g of cis N,N-dimethyl-5-[4-nitrophenoxy]-6,7,8,9-tetrahydro-benzocycloheptene-7-amine in 200 ml of ethanol and one liter of hydrogen was bubbled therethrough for 30 minutes with stirring. The mixture was filtered and the filtrate was evaporated to dryness under reduced pressure to obtain 3.6 g of cis N,N-dimethyl-5-[4-aminophenoxy]-6,7,8,9-tetrahydro-5H-benzocycloheptene-7-amine in the form of an orange oil. The said oil was dissolved in 20 ml of ethyl acetate and a solution of ethyl acetate saturated with gaseous hydrogen chloride was added thereto to adjust the pH to 1. The mixture stood for one hour at room temperature and was then vacuum filtered to obtain 4.1 g of the dihydrochloride of the cis compound in the form of colorless crystals melting at ≈260° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04177292 |
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| Source dataset | uspto-grants-1979_12 |
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| ORD ID | ord-d72f181dd1b04766b1328306636529e8 |
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| Source note | uspto-grants-1979_12 |
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